CN113782416A - HgCdTe liquid phase epitaxial growth source substrate, preparation method thereof and HgCdTe liquid phase epitaxial growth method - Google Patents
HgCdTe liquid phase epitaxial growth source substrate, preparation method thereof and HgCdTe liquid phase epitaxial growth method Download PDFInfo
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- CN113782416A CN113782416A CN202111070423.7A CN202111070423A CN113782416A CN 113782416 A CN113782416 A CN 113782416A CN 202111070423 A CN202111070423 A CN 202111070423A CN 113782416 A CN113782416 A CN 113782416A
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- 239000000758 substrate Substances 0.000 title claims abstract description 178
- 229910000661 Mercury cadmium telluride Inorganic materials 0.000 title claims abstract description 64
- 238000000034 method Methods 0.000 title claims abstract description 54
- 239000007791 liquid phase Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000007747 plating Methods 0.000 claims abstract description 109
- MCMSPRNYOJJPIZ-UHFFFAOYSA-N cadmium;mercury;tellurium Chemical compound [Cd]=[Te]=[Hg] MCMSPRNYOJJPIZ-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000013078 crystal Substances 0.000 claims abstract description 20
- 239000010413 mother solution Substances 0.000 claims abstract description 9
- 239000010410 layer Substances 0.000 claims description 101
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 98
- 239000000243 solution Substances 0.000 claims description 59
- 229910052793 cadmium Inorganic materials 0.000 claims description 52
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 49
- 229910052802 copper Inorganic materials 0.000 claims description 49
- 239000010949 copper Substances 0.000 claims description 49
- 229910052759 nickel Inorganic materials 0.000 claims description 49
- 238000000576 coating method Methods 0.000 claims description 44
- 239000011248 coating agent Substances 0.000 claims description 39
- 239000007921 spray Substances 0.000 claims description 36
- QWUZMTJBRUASOW-UHFFFAOYSA-N cadmium tellanylidenezinc Chemical compound [Zn].[Cd].[Te] QWUZMTJBRUASOW-UHFFFAOYSA-N 0.000 claims description 32
- 239000011247 coating layer Substances 0.000 claims description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 25
- 229910002804 graphite Inorganic materials 0.000 claims description 25
- 239000010439 graphite Substances 0.000 claims description 25
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- 238000000151 deposition Methods 0.000 claims description 24
- VCEXCCILEWFFBG-UHFFFAOYSA-N mercury telluride Chemical compound [Hg]=[Te] VCEXCCILEWFFBG-UHFFFAOYSA-N 0.000 claims description 19
- 238000005530 etching Methods 0.000 claims description 18
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 17
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 16
- 229910052753 mercury Inorganic materials 0.000 claims description 16
- 229910000570 Cupronickel Inorganic materials 0.000 claims description 14
- YOCUPQPZWBBYIX-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Cu] YOCUPQPZWBBYIX-UHFFFAOYSA-N 0.000 claims description 14
- 238000004070 electrodeposition Methods 0.000 claims description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
- 238000005507 spraying Methods 0.000 claims description 12
- 238000004943 liquid phase epitaxy Methods 0.000 claims description 10
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 9
- 229910052714 tellurium Inorganic materials 0.000 claims description 9
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims description 9
- 238000011049 filling Methods 0.000 claims description 7
- 238000011068 loading method Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 230000002194 synthesizing effect Effects 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 6
- 238000009718 spray deposition Methods 0.000 claims description 6
- 229910001431 copper ion Inorganic materials 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 9
- 230000005540 biological transmission Effects 0.000 abstract description 3
- 239000010409 thin film Substances 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 20
- 239000012452 mother liquor Substances 0.000 description 17
- 238000005406 washing Methods 0.000 description 16
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 12
- 239000003973 paint Substances 0.000 description 12
- 239000007788 liquid Substances 0.000 description 9
- 239000002131 composite material Substances 0.000 description 8
- 238000010586 diagram Methods 0.000 description 8
- 238000005498 polishing Methods 0.000 description 8
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 8
- 238000004140 cleaning Methods 0.000 description 7
- 238000000227 grinding Methods 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- OEDMOCYNWLHUDP-UHFFFAOYSA-N bromomethanol Chemical compound OCBr OEDMOCYNWLHUDP-UHFFFAOYSA-N 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 229910000365 copper sulfate Inorganic materials 0.000 description 5
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 230000000903 blocking effect Effects 0.000 description 4
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 4
- 229910001634 calcium fluoride Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 238000009713 electroplating Methods 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 235000013024 sodium fluoride Nutrition 0.000 description 4
- 239000011775 sodium fluoride Substances 0.000 description 4
- 239000002344 surface layer Substances 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000004781 supercooling Methods 0.000 description 2
- 229910004611 CdZnTe Inorganic materials 0.000 description 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000000861 blow drying Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000002059 diagnostic imaging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02551—Group 12/16 materials
- H01L21/02562—Tellurides
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/08—Electroplating with moving electrolyte e.g. jet electroplating
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/10—Electroplating with more than one layer of the same or of different metals
- C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/12—Semiconductors
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- H—ELECTRICITY
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
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- H01L21/02367—Substrates
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/02623—Liquid deposition
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a mercury cadmium telluride liquid phase epitaxial growth source substrate which comprises a substrate body and a complex plating layer, wherein the complex plating layer is arranged on the substrate body, and a window for liquid phase epitaxial growth of mercury cadmium telluride is arranged between the complex plating layer and the substrate body. Also discloses a preparation method of the HgCdTe liquid phase epitaxial growth source substrate and a HgCdTe liquid phase epitaxial growth method based on the substrate. The substrate can effectively solve the problems that the temperature of each point on an interface is reduced due to non-uniform temperature field and the heat conductivity coefficient of a transmission substrate material cannot well meet the temperature control conduction requirement before the mother solution is contacted with the substrate and in the epitaxial growth process of the HgCdTe thin film; the mercury cadmium telluride epitaxially grown on the substrate has good thickness uniformity, surface smoothness, high single crystal property and low half-peak width.
Description
Technical Field
The invention belongs to the technical field of mercury cadmium telluride liquid phase epitaxial growth, and particularly relates to a mercury cadmium telluride liquid phase epitaxial growth source substrate, a preparation method thereof and a substrate-based mercury cadmium telluride liquid phase epitaxial growth method.
Background
The tellurium-cadmium-mercury is an important II-VI group compound semiconductor, has excellent photoelectric performance, and the room-temperature nuclear radiation detector prepared by the tellurium-cadmium-mercury is widely applied to the fields of X-ray spectral analysis, medical imaging, industrial control, safety defense detection, basic scientific research and the like, and has wide application prospect and immeasurable market value.
The temperature in the liquid phase epitaxial growth source of the HgCdTe material has a large influence on the epitaxial growth rate, wherein the basic thermal conductivity of the substrate is a necessary requirement on the growth controllability of the HgCdTe material, when the substrate is just contacted, the temperature of an epitaxial system is near the crystallization temperature, the actual temperature of an interface can be higher or lower than the crystallization temperature due to non-uniform temperature fields, so that the phenomena of redissolution and supercooling growth can be caused, the crystallization temperature of mother liquor near the interface can be increased due to redissolution, the initial growth speed is accelerated due to supercooling, and the initial conditions of epitaxial growth are complicated, so that the temperature of each point on the interface and the thermal conductivity of the material of the transmission substrate cannot well meet the temperature control conduction requirement due to non-uniform temperature fields before the HgCdTe mother liquor is contacted with the substrate and in the epitaxial growth process of the HgCdTe thin film.
Disclosure of Invention
Aiming at the problems in the prior art, the substrate material of the HgCdTe liquid phase epitaxial growth source is provided in order to solve the problems that the temperature of each point on an interface can be reduced due to non-uniform temperature field before the mother solution is contacted with the substrate and in the process of the HgCdTe film epitaxial growth, and the heat conductivity coefficient of a transmission substrate material cannot well meet the temperature control conduction requirement.
In order to achieve the purpose, the invention adopts the following technical scheme:
a mercury cadmium telluride liquid phase epitaxial growth source substrate comprises a substrate body and a complex plating layer, wherein the complex plating layer is arranged on the substrate body, and a window for liquid phase epitaxial growth of mercury cadmium telluride is arranged between the complex plating layer and the substrate body. Namely, a window for the liquid phase epitaxial growth of mercury cadmium telluride is arranged on the complex plating layer, and the window extends to the surface of the substrate body.
Preferably, the complex plating layer is a multi-layer complex plating layer; preferably, the multilayer complex plating layer is a copper/nickel complex plating layer; preferably, the thickness of the multilayer complex plating layer is 50-100 mu m; preferably, the molar ratio of copper to nickel in the copper/nickel complex plating layer is 2-10: 5-8.
Preferably, the copper/nickel complex plating layer is a complex plating layer formed by alternating copper and nickel; the copper/nickel complex plating layer is formed by alternately depositing a copper layer and a nickel layer on a cadmium zinc telluride substrate by a spray electrodeposition method.
Preferably, the substrate body is a cadmium zinc telluride substrate; the resistivity of the cadmium zinc telluride substrate is 108-148 omega-m.
As a general inventive concept, a preparation method of the mercury cadmium telluride liquid phase epitaxial growth source substrate is also provided, which comprises the following steps:
(1) preparing a substrate body;
(2) coating a fluoride coating layer on a lattice growth surface area of the substrate body for epitaxial growth of mercury cadmium telluride;
(3) depositing a complex coating on the surfaces of the substrate body and the fluoride coating layer;
(4) and removing the complex plating layer and the fluoride coating layer corresponding to the lattice growth surface region, and forming a window for epitaxial growth of mercury cadmium telluride on the substrate body.
Preferably, in the step (3), the complex plating layer is a multi-layer complex plating layer, and the multi-layer complex plating layer is a copper/nickel complex plating layer; the multilayer complex coating is alternately deposited on the tellurium-zinc-cadmium substrate body and the fluoride coating layer by a spray electrodeposition method; the deposition method of the multilayer complex plating layer specifically comprises the following steps: respectively adding the prepared copper solution and nickel solution into corresponding plating solution spray heads, then spraying the copper solution and the nickel solution to the surfaces of the tellurium-zinc-cadmium substrate body and the fluoride coating layer through the spray heads, and repeatedly and alternately spraying and depositing to form a copper and nickel complex plating layer; (ii) a The thickness of the spray deposition is 50-100 mu m.
Preferably, in the step (2), the fluoride coating layer is coated by using a mask process, and the method specifically comprises the following steps: covering a lattice growth surface area except for the tellurium, cadmium and mercury epitaxially grown on the substrate body by using a mask plate, and then coating a fluoride coating layer on the lattice growth surface area.
In the step (1), the substrate body is a cadmium zinc telluride substrate; the preparation of the substrate comprises: and grinding and polishing the crystal phase surface of the tellurium-zinc-cadmium substrate 111 by using 1% bromomethanol, then washing by using an isopropanol solution and drying by using a nitrogen gun.
Preferably, in the step (4), etching the copper-nickel complex plating layer on the lattice surface of the region to be grown on the surface of the substrate by using an etching solution, wherein the etching solution is an aqueous solution of hydrochloric acid, nitric acid and a cupric ion source, the mass percent of the hydrochloric acid is 10-15%, the mass percent of the nitric acid is 1-10%, the mass percent of the cupric ion is 0.001-0.01%, the cupric ion source can be provided by copper sulfate or copper oxide, fluoride is removed by distillation with distilled water at 130-135 ℃, and after removal, the copper-nickel complex plating layer can be cleaned by using an organic solvent, and the organic solvent is acetone, absolute ethyl alcohol and methanol.
Preferably, the area coated with the fluorinated coating is positioned at the center of the crystal lattice growth 111 plane on the surface of the substrate body.
As a general inventive concept, the invention also provides a mercury cadmium telluride liquid phase epitaxial growth method, which comprises the following steps:
s1, loading the tellurium-cadmium-mercury liquid phase epitaxial growth source substrate or the tellurium-cadmium-mercury liquid phase epitaxial growth source substrate prepared by the preparation method into an epitaxial graphite boat;
s2, synthesizing an epitaxial mother solution by using tellurium, cadmium and mercury as raw materials, compensating by using mercury telluride as mercury, and filling an appropriate amount of epitaxial mother solution and mercury telluride into an epitaxial graphite boat;
and S3, controlling the initial temperature field and the growth process temperature field of the graphite boat to enable the epitaxial mother solution to carry out liquid phase epitaxy on the surface of the substrate lattice plane.
Preferably, step S1 further includes cleaning the te-cd-hg liquid-phase epitaxial growth source substrate with an organic solvent, where the organic solvent is acetone, absolute ethyl alcohol, and methanol.
Compared with the prior art, the invention has the following advantages:
in the invention, the copper and nickel multilayer complex plating film is prepared on the tellurium-zinc-cadmium liner substrate by using a jet electrodeposition method, so that the temperature field control capability of the tellurium-cadmium-mercury mother solution in contact with the substrate can be effectively improved when the tellurium-cadmium-mercury liquid-phase epitaxial growth source is operated, the uniform heat conduction processing capability of each point on the surface of the substrate is ensured, the requirement on temperature control conduction can be met, and the improvement of the surface integrity of the tellurium-cadmium-mercury film through temperature control is facilitated; the prepared complex plating layer can enable the tellurium-zinc-cadmium gasket substrate to have higher hardness, stronger corrosion resistance and better wear resistance, thereby realizing the enhancement of the physical strength of the tellurium-cadmium-mercury gasket through the copper-nickel multilayer complex film and improving the corresponding mechanical property. The tellurium-cadmium-mercury epitaxial film grown by the substrate liquid phase epitaxy has quite good thickness uniformity, surface smoothness, high single crystal property and lower half-peak width.
Drawings
FIG. 1 is a block diagram of a liquid phase epitaxial growth source substrate process flow of the present invention.
FIG. 2 is a diagram of a substrate preparation structure of a liquid phase epitaxial growth source of the present invention.
FIG. 3 is a schematic diagram of the processing of the multi-layer complex layer of the CdZnTe substrate according to the present invention.
FIG. 4 is a coated block fluorinated coating reticle.
In fig. 5, (a) is a test chart of the surface flatness of the epitaxial film of mercury cadmium telluride obtained in example 3, and (b) is a test chart of the surface flatness of the epitaxial film of mercury cadmium telluride obtained in comparative example 1.
Reference numerals:
1. copper-nickel complex plating; 2. fluoridizing the coating layer; 3. a cadmium zinc telluride substrate; 4. copper and nickel plating solution spray heads.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The substrate of the mercury cadmium telluride liquid phase epitaxial growth source comprises a cadmium zinc telluride substrate and a plurality of layers of complex coatings, wherein the plurality of layers of complex coatings are loaded on the top of a cadmium zinc telluride substrate body, the plurality of layers of complex coatings are alternately deposited on the top of the cadmium zinc telluride substrate body through a jet electrodeposition method, the plurality of layers of complex coatings are copper/nickel complex coatings, the molar ratio of copper to nickel is 2:8, the substrate body is the cadmium zinc telluride substrate, the size of cadmium zinc telluride is 2cm multiplied by 3cm, and the resistivity of the cadmium zinc telluride substrate is 108-148 omega.
The substrate of the mercury cadmium telluride liquid phase epitaxial growth source has a specific process flow diagram as shown in figure 1, and the preparation method comprises the following steps:
(1) the method for preparing the tellurium-zinc-cadmium substrate comprises the following specific processing steps: grinding, polishing, grinding and polishing 111 crystal phase surfaces of the cadmium zinc telluride substrate by using 1% bromomethanol, then washing by using an isopropanol solution, blow-drying by using a nitrogen gun, arranging a certain oxygen pressure outside electroplating equipment, and performing spray electrodeposition on a copper and nickel multilayer complex film by using the cadmium zinc telluride substrate as a base, wherein the resistivity of the cadmium zinc telluride substrate is 108-148 omega.m;
(2) adopting a mask to shield, and coating a fluorinated coating layer on the crystal lattice growth surface on the surface of the substrate body; the coating fluorinated paint is positioned at the center of a 111 plane of the crystal lattice growth on the surface of the cadmium zinc telluride substrate, the area of the coating fluorinated paint is 1.6cm multiplied by 2.4cm, the coating blocking fluorinated paint is blocked by a mask plate, the length, the width and the height of the mask plate are respectively 3.2cm, 2.2cm and 2cm, and the coating area is 1.6cm multiplied by 2.4cm, as shown in figure 4; the fluoride may be calcium fluoride or sodium fluoride.
(3) Depositing a tellurium-zinc-cadmium substrate multilayer complex coating, wherein a processing schematic diagram of processing and depositing the tellurium-zinc-cadmium substrate multilayer complex coating is shown in FIG. 3, and the processing and depositing method specifically comprises the following steps: respectively adding the prepared copper solution and nickel solution into corresponding plating solution spray heads, spraying the composite plating solution to the surface of the substrate body and the surface of the fluorinated coating layer through the spray heads of the spray gun, controlling the linear reciprocating motion of the base by the spray gun through a plating solution platform driving piece, and repeatedly performing alternate spraying and deposition on the two-side liquid dropping spray heads to form the composite plating solution; the thickness of the spray deposition is 50-100 mu m of copper and nickel complex plating layer, so that the copper and nickel complex plating layer is sprayed on the surface of the substrate body and the surface of the fluorinated coating layer, and the obtained substrate preparation structure chart is shown in figure 2; the copper-nickel complex plating layer on the lattice surface of the area to be grown on the surface of the substrate is etched and corroded by using an etching solution, the etching solution is aqueous solution of hydrochloric acid, nitric acid and a cupric ion source, wherein the mass percent of the hydrochloric acid is 10-15%, the mass percent of the nitric acid is 1-10%, the mass percent of the cupric ion is 0.001-0.01%, the cupric ion source is provided by using copper sulfate, the copper-nickel complex plating layer surface layer in the growth range is removed by using the etching solution, then fluoride is removed by using a distillation method, distilled water is used for washing, then alcohol and acetone are used for washing, and the corresponding growth lattice surface is exposed by washing.
The mercury cadmium telluride liquid phase epitaxial growth method based on the mercury cadmium telluride liquid phase epitaxial growth source substrate specifically comprises the following steps:
s1, improving the corresponding thickness of the epitaxial graphite boat according to the thickness of the multi-layer complex plating tellurium-zinc-cadmium substrate;
s2, cleaning the tellurium-zinc-cadmium substrate layer and then loading the cleaned substrate layer into an epitaxial graphite boat;
s3, synthesizing the epitaxial mother liquor by using tellurium, cadmium and mercury as raw materials, compensating the mercury by using mercury telluride, weighing proper amount of epitaxial mother liquor and mercury telluride, and filling the epitaxial mother liquor and the mercury telluride into an epitaxial graphite boat for liquid phase epitaxy;
s4, controlling the initial temperature field and the growth process temperature field of the graphite boat, and forming the mercury cadmium telluride epitaxial film by the epitaxial mother liquid.
Example 2
In one embodiment, the invention also provides a tellurium-zinc-cadmium liquid phase epitaxial growth source substrate, which comprises a tellurium-zinc-cadmium substrate and a multilayer complex plating layer, wherein the multilayer complex plating layer is loaded on the top of the tellurium-zinc-cadmium substrate, the multilayer complex plating layer is alternately deposited on the top of the tellurium-zinc-cadmium substrate through a spray electrodeposition method, the multilayer complex plating layer is a copper/nickel complex plating layer, and the molar ratio of copper to nickel is 4: 6.
The preparation method of the substrate of the mercury cadmium telluride liquid phase epitaxial growth source comprises the following steps:
(1) the method for preparing the tellurium-zinc-cadmium substrate comprises the following specific processing steps: grinding and polishing a 111 crystal phase surface of the cadmium zinc telluride substrate by using 1% bromomethanol, then washing by using an isopropanol solution, drying by using a nitrogen gun, arranging a certain oxygen pressure outside electroplating equipment, and performing spray electrodeposition on a copper and nickel multilayer complex film by using the cadmium zinc telluride substrate as a base, wherein the resistivity of the cadmium zinc telluride substrate is 108-148 omega.
(2) Adopting a mask to shield, and coating a fluorinated coating layer on the crystal lattice growth surface on the surface of the substrate body; the coating fluorinated paint is positioned at the center of a 111 plane of the crystal lattice growth on the surface of the cadmium zinc telluride substrate, the area of the coating fluorinated paint is 1.6cm multiplied by 2.4cm, the coating blocking fluorinated paint is blocked by a mask plate, the length, the width and the height of the mask plate are respectively 3.2cm, 2.2cm and 2cm, and the coating area is 1.6cm multiplied by 2.4cm, as shown in figure 4; the fluoride may be calcium fluoride or sodium fluoride.
(3) Depositing a tellurium-zinc-cadmium substrate multilayer complex coating, wherein a processing schematic diagram of processing and depositing the tellurium-zinc-cadmium substrate multilayer complex coating is shown in FIG. 3, and the processing and depositing method specifically comprises the following steps: respectively adding the prepared copper solution and nickel solution into corresponding plating solution spray heads, spraying the composite plating solution to the surface of the substrate body and the surface of the fluorinated coating layer through the spray heads of the spray gun, controlling the linear reciprocating motion of the base by the spray gun through a plating solution platform driving piece, and repeatedly performing alternate spraying and deposition on the two-side liquid dropping spray heads to form the composite plating solution; the thickness of the spray deposition is 50-100 mu m of copper and nickel complex plating layer, so that the copper and nickel complex plating layer is sprayed on the surface of the substrate body and the surface of the fluorinated coating layer, and the obtained substrate preparation structure chart is shown in figure 2; the copper-nickel complex plating layer on the lattice surface of the area to be grown on the surface of the substrate is etched and corroded by using an etching solution, the etching solution is aqueous solution of hydrochloric acid, nitric acid and a cupric ion source, wherein the mass percent of the hydrochloric acid is 10-15%, the mass percent of the nitric acid is 1-10%, the mass percent of the cupric ion is 0.001-0.01%, the cupric ion source is provided by using copper sulfate, the copper-nickel complex plating layer surface layer in the growth range is removed by using the etching solution, then fluoride is removed by using a distillation method, distilled water is used for washing, then alcohol and acetone are used for washing, and the corresponding growth lattice surface is exposed by washing.
The mercury cadmium telluride liquid phase epitaxial growth method specifically comprises the following steps:
s1, improving the corresponding thickness of the epitaxial graphite boat according to the thickness of the multi-layer complex plating tellurium-zinc-cadmium substrate;
s2, cleaning the multilayer complex plating tellurium-zinc-cadmium substrate, cleaning and then loading into an epitaxial graphite boat;
s3, synthesizing the epitaxial mother liquor by using tellurium, cadmium and mercury as raw materials, compensating the mercury by using mercury telluride, weighing proper amount of epitaxial mother liquor and mercury telluride, and filling the epitaxial mother liquor and the mercury telluride into an epitaxial graphite boat for liquid phase epitaxy;
s4, controlling the initial temperature field and the growth process temperature field of the graphite boat, and forming the mercury cadmium telluride epitaxial film by the epitaxial mother liquid.
Example 3
In one embodiment, the invention also provides a substrate material of the tellurium-zinc-cadmium liquid phase epitaxial growth source, which comprises a tellurium-zinc-cadmium substrate and a multilayer complex plating layer, wherein the multilayer complex plating layer is loaded on the top of the tellurium-zinc-cadmium substrate, the multilayer complex plating layer is alternately deposited on the top of the tellurium-zinc-cadmium substrate through a spray electrodeposition method, the multilayer complex plating layer is a copper/nickel complex plating layer, and the molar ratio of copper to nickel is 7: 5.
The preparation method of the substrate of the mercury cadmium telluride liquid phase epitaxial growth source comprises the following steps:
(1) the method for preparing the tellurium-zinc-cadmium substrate comprises the following specific processing steps: grinding and polishing a 111 crystal phase surface of the cadmium zinc telluride substrate by using 1% bromomethanol, then washing by using an isopropanol solution, drying by using a nitrogen gun, arranging a certain oxygen pressure outside electroplating equipment, and performing spray electrodeposition on a copper and nickel multilayer complex film by using the cadmium zinc telluride substrate as a base, wherein the resistivity of the cadmium zinc telluride substrate is 108-148 omega.
(2) Adopting a mask to shield, and coating a fluorinated coating layer on the crystal lattice growth surface on the surface of the substrate body; the coating fluorinated paint is positioned at the center of a 111 plane of the crystal lattice growth on the surface of the cadmium zinc telluride substrate, the area of the coating fluorinated paint is 1.6cm multiplied by 2.4cm, the coating blocking fluorinated paint is blocked by a mask plate, the length, the width and the height of the mask plate are respectively 3.2cm, 2.2cm and 2cm, and the coating area is 1.6cm multiplied by 2.4cm, as shown in figure 4; the fluoride may be calcium fluoride or sodium fluoride.
(3) Depositing a tellurium-zinc-cadmium substrate multilayer complex coating, wherein a processing schematic diagram of processing and depositing the tellurium-zinc-cadmium substrate multilayer complex coating is shown in FIG. 3, and the processing and depositing method specifically comprises the following steps: respectively adding the prepared copper solution and nickel solution into corresponding plating solution spray heads, spraying the composite plating solution to the surface of the substrate body and the surface of the fluorinated coating layer through the spray heads of the spray gun, controlling the linear reciprocating motion of the base by the spray gun through a plating solution platform driving piece, and repeatedly performing alternate spraying and deposition on the two-side liquid dropping spray heads to form the composite plating solution; the thickness of the spray deposition is 50-100 mu m of copper and nickel complex plating layer, so that the copper and nickel complex plating layer is sprayed on the surface of the substrate body and the surface of the fluorinated coating layer, and the obtained substrate preparation structure chart is shown in figure 2; the copper-nickel complex plating layer on the lattice surface of the area to be grown on the surface of the substrate is etched and corroded by using an etching solution, the etching solution is aqueous solution of hydrochloric acid, nitric acid and a cupric ion source, wherein the mass percent of the hydrochloric acid is 10-15%, the mass percent of the nitric acid is 1-10%, the mass percent of the cupric ion is 0.001-0.01%, the cupric ion source is provided by using copper sulfate, the copper-nickel complex plating layer surface layer in the growth range is removed by using the etching solution, then fluoride is removed by using a distillation method, distilled water is used for washing, then alcohol and acetone are used for washing, and the corresponding growth lattice surface is exposed by washing.
The mercury cadmium telluride liquid phase epitaxial growth method specifically comprises the following steps:
s1, improving the corresponding thickness of the epitaxial graphite boat according to the thickness of the multi-layer complex plating tellurium-zinc-cadmium substrate;
s2, cleaning the multilayer complex plating tellurium-zinc-cadmium substrate, and then loading the substrate into an epitaxial graphite boat;
s3, synthesizing the epitaxial mother liquor by using tellurium, cadmium and mercury as raw materials, compensating the mercury by using mercury telluride, weighing proper amount of epitaxial mother liquor and mercury telluride, and filling the epitaxial mother liquor and the mercury telluride into an epitaxial graphite boat for liquid phase epitaxy;
s4, controlling the initial temperature field and the growth process temperature field of the graphite boat, and forming the mercury cadmium telluride epitaxial film by the epitaxial mother liquid.
Example 4
In one embodiment, the invention also provides a substrate material of the tellurium-zinc-cadmium liquid phase epitaxial growth source, which comprises a tellurium-zinc-cadmium substrate and a multilayer complex plating layer, wherein the multilayer complex plating layer is loaded on the top of the tellurium-zinc-cadmium substrate, the multilayer complex plating layer is alternately deposited on the top of the tellurium-zinc-cadmium substrate through a spray electrodeposition method, the multilayer complex plating layer is a copper/nickel complex plating layer, and the molar ratio of copper to nickel is 10: 5.
The preparation method of the substrate of the mercury cadmium telluride liquid phase epitaxial growth source comprises the following steps:
(1) the method for preparing the tellurium-zinc-cadmium substrate comprises the following specific processing steps: grinding and polishing a 111 crystal phase surface of the cadmium zinc telluride substrate by using 1% bromomethanol, then washing by using an isopropanol solution, drying by using a nitrogen gun, arranging a certain oxygen pressure outside electroplating equipment, and performing spray electrodeposition on a copper and nickel multilayer complex film by using the cadmium zinc telluride substrate as a base, wherein the resistivity of the cadmium zinc telluride substrate is 108-148 omega.
(2) Adopting a mask to shield, and coating a fluorinated coating layer on the crystal lattice growth surface on the surface of the substrate body; the coating fluorinated paint is positioned at the center of a 111 plane of the crystal lattice growth on the surface of the cadmium zinc telluride substrate, the area of the coating fluorinated paint is 1.6cm multiplied by 2.4cm, the coating blocking fluorinated paint is blocked by a mask plate, the length, the width and the height of the mask plate are respectively 3.2cm, 2.2cm and 2cm, and the coating area is 1.6cm multiplied by 2.4cm, as shown in figure 4; the fluoride may be calcium fluoride or sodium fluoride.
(3) Depositing a tellurium-zinc-cadmium substrate multilayer complex coating, wherein a processing schematic diagram of processing and depositing the tellurium-zinc-cadmium substrate multilayer complex coating is shown in FIG. 3, and the processing and depositing method specifically comprises the following steps: respectively adding the prepared copper solution and nickel solution into corresponding plating solution spray heads, spraying the composite plating solution to the surface of the substrate body and the surface of the fluorinated coating layer through the spray heads of the spray gun, controlling the linear reciprocating motion of the base by the spray gun through a plating solution platform driving piece, and repeatedly performing alternate spraying and deposition on the two-side liquid dropping spray heads to form the composite plating solution; the thickness of the spray deposition is 50-100 mu m of copper and nickel complex plating layer, so that the copper and nickel complex plating layer is sprayed on the surface of the substrate body and the surface of the fluorinated coating layer, and the obtained substrate preparation structure chart is shown in figure 2; the copper-nickel complex plating layer on the lattice plane of the area to be grown on the surface of the substrate is etched and corroded by using an etching solution, the etching solution is an aqueous solution of hydrochloric acid, nitric acid and a cupric ion source, wherein the mass percent of the hydrochloric acid is 10-15%, the mass percent of the nitric acid is 1-10%, the mass percent of the cupric ion is 0.001-0.01%, the cupric ion source is provided by using copper sulfate, the copper-nickel complex plating layer surface layer in the growth range is removed by using the etching solution, then the fluoride is removed by using a distillation method and is washed by using distilled water, then the copper-nickel complex plating layer is washed by using alcohol and acetone, and the corresponding growth lattice plane is exposed by washing.
The mercury cadmium telluride liquid phase epitaxial growth method specifically comprises the following steps:
s1, improving the corresponding thickness of the epitaxial graphite boat according to the thickness of the multi-layer complex plating tellurium-zinc-cadmium substrate;
s2, cleaning the multilayer complex plating tellurium-zinc-cadmium substrate, and then loading the substrate into an epitaxial graphite boat;
s3, synthesizing the epitaxial mother liquor by using tellurium, cadmium and mercury as raw materials, compensating the mercury by using mercury telluride, weighing proper amount of epitaxial mother liquor and mercury telluride, and filling the epitaxial mother liquor and the mercury telluride into an epitaxial graphite boat for liquid phase epitaxy;
s4, controlling the initial temperature field and the growth process temperature field of the graphite boat, and forming the mercury cadmium telluride epitaxial film by the epitaxial mother liquid.
Comparative example 1
A substrate of a tellurium-zinc-cadmium liquid phase epitaxial growth source is a tellurium-zinc-cadmium substrate.
The method for processing the tellurium-zinc-cadmium substrate specifically comprises the following steps: grinding and polishing a 111 crystal phase surface of a cadmium zinc telluride substrate by using 1% bromomethanol, then washing by using an isopropanol solution and drying by using a nitrogen gun, wherein the resistivity of the cadmium zinc telluride substrate is 108-148 omega-m;
the crystal lattice growth surface of the tellurium-zinc-cadmium substrate is 111 surfaces, and the area of the crystal lattice growth surface is 2cm multiplied by 3 cm.
The mercury cadmium telluride liquid phase epitaxial growth method specifically comprises the following steps:
s1, cleaning the cadmium zinc telluride substrate and then loading the substrate into an epitaxial graphite boat;
s2, synthesizing the epitaxial mother liquor by using tellurium, cadmium and mercury as raw materials, compensating the mercury by using mercury telluride, weighing proper amount of epitaxial mother liquor and mercury telluride, and filling the epitaxial mother liquor and the mercury telluride into an epitaxial graphite boat for liquid phase epitaxy;
s3, controlling the initial temperature field and the growth process temperature field of the graphite boat, and forming the mercury cadmium telluride epitaxial film by the epitaxial mother liquid.
The prepared epitaxial films of mercury cadmium telluride were characterized as shown in fig. 5, where (a) is a test chart of the surface flatness of the epitaxial film of mercury cadmium telluride obtained by liquid phase epitaxy in example 3, and (b) is a test chart of the surface flatness of the epitaxial film of mercury cadmium telluride obtained by liquid phase epitaxy in comparative example 1, and it can be seen from fig. 5 that the flatness of the epitaxial film of mercury cadmium telluride obtained by epitaxial growth was significantly improved compared with the substrate without the alloy plating layer.
The thickness of the work pieces before and after the electrodeposition of the epitaxial growth source substrates prepared in examples 1 to 4 and comparative example 1 was measured with a laser thickness gauge to calculate the thickness of the plating layer, the friction factor of the plated layer after polishing was measured and compared with a friction wear tester, and the amount of wear was weighed to calculate the amount of wear, and the corresponding thermal conductivity was measured, and the measured performance parameters were as shown in table 1:
TABLE 1
As can be seen from the above table, in example 3 which is a preferred embodiment of the present invention, in the case that the molar ratio of copper to nickel is 7:5, the thermal conductivity, the thickness of the plating layer, the relative mean square deviation of the surface distribution of the material components, and the relative mean square deviation of the thickness are all better processed, and the transmittance measured by an infrared fourier spectrometer reaches 56%.
While the invention has been described with reference to specific preferred embodiments, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The mercury cadmium telluride liquid phase epitaxial growth source substrate is characterized by comprising a substrate body and a complex plating layer, wherein the complex plating layer is arranged on the substrate body, and a window for liquid phase epitaxial growth of mercury cadmium telluride is arranged between the complex plating layer and the substrate body.
2. The mercury cadmium telluride liquid phase epitaxial growth source substrate of claim 1, wherein the complex plating layer is a multilayer complex plating layer; the multilayer complex plating layer is a copper/nickel complex plating layer; the thickness of the multi-layer complex plating layer is 50-100 mu m; the molar ratio of copper to nickel in the copper/nickel complex plating layer is 2-10: 5-8.
3. The mercury cadmium telluride liquid phase epitaxial growth source substrate of claim 2, wherein the copper/nickel complex plating layer is a complex plating layer in which copper and nickel are alternated; the copper/nickel complex plating layer is formed by alternately depositing a copper layer and a nickel layer on a cadmium zinc telluride substrate by a spray electrodeposition method.
4. The HgCdTe liquid phase epitaxial growth source substrate of any one of claims 1-3, wherein the substrate body is a HgCdTe substrate; the resistivity of the cadmium zinc telluride substrate is 108-148 omega-m.
5. The method for preparing a mercury cadmium telluride liquid phase epitaxial growth source substrate as claimed in any one of claims 1 to 4, comprising the steps of:
(1) preparing a substrate body;
(2) coating a fluoride coating layer on a lattice growth surface area of the substrate body for epitaxial growth of mercury cadmium telluride;
(3) depositing a complex coating on the surfaces of the substrate body and the fluoride coating layer;
(4) and removing the complex plating layer and the fluoride coating layer corresponding to the lattice growth surface region, and forming a window for epitaxial growth of mercury cadmium telluride on the substrate body.
6. The method for preparing a mercury cadmium telluride liquid phase epitaxial growth source substrate according to claim 5, wherein in the step (3), the complex plating layer is a multi-layer complex plating layer, and the multi-layer complex plating layer is a copper/nickel complex plating layer; the multilayer complex coating is alternately deposited on the tellurium-zinc-cadmium substrate body and the fluoride coating layer by a spray electrodeposition method; the deposition method of the multilayer complex plating layer specifically comprises the following steps: respectively adding the prepared copper solution and nickel solution into corresponding plating solution spray heads, then spraying the copper solution and the nickel solution to the surfaces of the tellurium-zinc-cadmium substrate body and the fluoride coating layer through the spray heads, and repeatedly and alternately spraying and depositing to form a complex plating layer of copper and nickel; the thickness of the spray deposition is 50-100 mu m.
7. The method for preparing a mercury cadmium telluride liquid phase epitaxial growth source substrate according to claim 5, wherein in the step (2), the fluoride coating layer is coated by adopting a mask process, and the method specifically comprises the following steps: covering a lattice growth surface area except for the tellurium, cadmium and mercury epitaxially grown on the substrate body by using a mask plate, and then coating a fluoride coating layer on the lattice growth surface area.
8. The method for preparing the mercury cadmium telluride liquid phase epitaxial growth source substrate according to claim 5, wherein the area coated with the fluorinated coating is positioned at the center of the 111 plane of the crystal lattice growth on the surface of the substrate body.
9. The method for preparing the HgCdTe liquid phase epitaxial growth source substrate according to claim 5, wherein in the step (4), the copper-nickel complex plating layer on the lattice surface of the region to be grown on the surface of the substrate is etched and corroded by using an etching solution, and the etching solution is an aqueous solution of hydrochloric acid, nitric acid and a cupric ion source; in the etching solution, the mass percent of hydrochloric acid is 10-15%, the mass percent of nitric acid is 1-10%, and the mass percent of divalent copper ions is 0.001-0.01%; the fluoride is removed by distillation.
10. A mercury cadmium telluride liquid phase epitaxial growth method is characterized by comprising the following steps:
s1, loading the mercury cadmium telluride liquid phase epitaxial growth source substrate as defined in any one of claims 1 to 4 or the mercury cadmium telluride liquid phase epitaxial growth source substrate prepared by the preparation method as defined in any one of claims 5 to 9 into an epitaxial graphite boat;
s2, synthesizing an epitaxial mother solution by using tellurium, cadmium and mercury as raw materials, compensating by using mercury telluride as mercury, and filling an appropriate amount of epitaxial mother solution and mercury telluride into an epitaxial graphite boat;
and S3, controlling the initial temperature field and the growth process temperature field of the graphite boat to enable the epitaxial mother solution to carry out liquid phase epitaxy on the surface of the substrate lattice plane.
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